CN212769857U - Hydrochloric acid resolving device with negative pressure dehydration function - Google Patents
Hydrochloric acid resolving device with negative pressure dehydration function Download PDFInfo
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Abstract
The utility model provides a hydrochloric acid desorption device with negative pressure dehydration function, which comprises a desorption device and a negative pressure dehydration device, wherein the desorption device comprises a desorption tower, a three-stage preheater, a desorption tower condenser, a demister, a desorption tower reboiling device and a desorption tower dilute acid buffer tank; the negative pressure dehydration device is communicated with the dilute acid buffer tank of the desorption tower through a pipeline and comprises a negative pressure dehydration tower, a dilute acid buffer tank of the dehydration tower, a condenser of the dehydration tower, a vacuum unit, a dilute acid water tank and a dehydration reboiling device. The utility model discloses a hydrochloric acid desorption device with negative pressure dehydration function, with the analytic technology combination of negative pressure dehydration technology and hydrochloric acid, compare reduction equipment investment and the running cost that can be great with the design of traditional components of a whole that can function independently technology, simultaneously can improve the utilization ratio of the energy through reasonable design, the utility model discloses an analytic technology of hydrochloric acid does not receive impurity influence in the raw materials hydrochloric acid of pending processing, compares 15 ~ 50% comprehensive energy consumption of saving with the design of current components of a whole that can function independently.
Description
Technical Field
The utility model relates to an analytic technical field of hydrochloric acid, concretely relates to analytic device of hydrochloric acid with negative pressure dehydration function.
Background
In industrial production, concentrated hydrochloric acid is often required to be resolved to produce HCL gas, and then the resolved diluted hydrochloric acid is returned to the production process to absorb HCL to generate concentrated hydrochloric acid so as to maintain the production balance of a factory, and when the balance does not contain other impurities (including organic matters, metal ions, water and the like), the material balance of a production system can be maintained through conventional resolution. However, in the actual plant production, when hydrochloric acid after being used and analyzed is returned to the production process to absorb tail gas containing HCL, the tail gas often contains water and is absorbed together during absorption, and at this time, redundant water needs to be removed synchronously.
Dilute hydrochloric acid may also be used directly in some manufacturing processes as a solvent or feedstock, where acidic waste water containing numerous impurities may be produced, and excess water may be removed to maintain manufacturing balance.
The conventional hydrochloric acid can only resolve part of HCL in the concentrated hydrochloric acid by normal resolution, and meanwhile, the azeotropic acid is a byproduct. The removal of the excess water in hydrochloric acid in industrial production requires deep analysis, which is generally divided into an extractive distillation method and a pressure difference method. The extractive distillation methods are divided into calcium chloride and sulfuric acid methods. Because the sulfuric acid has strong corrosivity and great difficulty in transportation, storage and operation, the sulfuric acid method has few application examples; calcium chloride is low in price and easy to obtain, so that the calcium chloride is relatively common in application, the calcium chloride is easy to crystallize due to too high concentration control, pipelines can be blocked in actual production due to improper operation, and if impurities (such as sulfate radicals, silicon dioxide and the like) are contained in hydrochloric acid, precipitates or deterioration can be generated, so that the calcium chloride is frequently replaced or supplemented after being recycled for a certain time, and waste is generated; the application case of the differential pressure method is general, although the analysis effect is good, the energy consumption is high, the investment is large, and the material balance control requirement of the device operation is high.
At present, an industrial device is generally independently arranged for normal analysis and deep analysis, the amount of the normal analysis of certain hydrochloric acid is large, and a factory with small removal amount of redundant water can increase investment, improve maintenance and operation cost and form energy waste if the normal analysis and the deep analysis are independently arranged, and particularly, the hydrochloric acid to be treated contains impurities such as lower alcohol, calcium, silicon dioxide and the like, is not suitable for the conditions of selecting a calcium chloride (or magnesium chloride) and a sulfuric acid method, and has very obvious energy-saving effect.
Similar plants include, but are not limited to: the industries of synthesizing polyvinyl chloride, gas-phase white carbon black, burning of chlorine-containing tail gas, certain pharmaceutical and pesticide intermediates and the like have the conditions of large hydrochloric acid desorption amount and small water removal amount, and the hydrochloric acid contains some impurities which are deeply desorbed and sensitive by adopting a common calcium chloride and sulfuric acid method. How to utilize hydrochloric acid normal analytic device's condition desorption a certain amount of water through technology optimization to retrieve low boiling organic matter, still need reach more energy-conserving purpose than prior art means simultaneously, it is the utility model discloses the problem of research solution.
SUMMERY OF THE UTILITY MODEL
In order to solve the problem, the utility model provides a hydrochloric acid desorption device with negative pressure dehydration function, with the analytic technology combination of negative pressure dehydration technology and hydrochloric acid, with unnecessary water removal at the analytic in-process of hydrochloric acid, compare with traditional components of a whole that can function independently process design, reduction equipment investment and running cost that can be great can improve the utilization ratio of the energy through reasonable design simultaneously, the utility model discloses an analytic technology of hydrochloric acid does not receive impurity influence in the pending raw materials hydrochloric acid, compares with current components of a whole that can function independently design and practices thrift 15 ~ 50% comprehensive energy consumption efficiency.
In order to achieve the above purpose, the utility model discloses a technical scheme who takes is:
a hydrochloric acid desorption device with a negative pressure dehydration function comprises a desorption device and a negative pressure dehydration device, wherein the desorption device comprises a desorption tower, a desorption tower condenser, a demister, a desorption tower reboiling device and a desorption tower diluted acid buffer tank, the top of the desorption tower condenser is communicated with the top of the desorption tower through a pipeline, the lower part of the demister is communicated with the desorption tower condenser through a pipeline, dried hydrogen chloride gas is output through the pipeline at the top of the demister, the bottom of the desorption tower condenser and the lower part of the demister are communicated with the upper part of the desorption tower through pipelines, the top of the desorption tower reboiling device is communicated with the lower part of the desorption tower through a pipeline, and the upper part of the desorption tower diluted acid buffer tank is communicated with the lower part of the desorption tower and the bottom of the desorption tower through pipelines; the negative pressure dehydration device, through the pipeline with the bottom intercommunication of analysis tower diluted acid buffer tank, the negative pressure dehydration device include negative pressure dehydration tower, dehydration tower diluted acid buffer tank, dehydration tower condenser, vacuum unit, diluted acid water pitcher and dehydration reboiling device, the upper portion of negative pressure dehydration tower pass through the pipeline with the bottom intercommunication of analysis tower diluted acid buffer tank, the lower part of dehydration tower diluted acid buffer tank with the bottom intercommunication of negative pressure dehydration tower, the top of dehydration tower condenser pass through the pipeline with the top intercommunication of negative pressure dehydration tower, the vacuum unit pass through the pipeline with the lower part intercommunication of dehydration tower condenser, the diluted acid water pitcher pass through the pipeline with the bottom intercommunication of dehydration tower condenser, the dehydration reboiling device pass through the pipeline with the lower part and the bottom intercommunication of negative pressure dehydration tower.
Further, still include waste heat recovery device, including one-level pre-heater, second grade pre-heater and tertiary pre-heater, dilute acid in the dehydration tower dilute acid buffer tank is in export to the hydrogen chloride absorption process through analytic tower dilute acid cooler behind the heat transfer in the one-level pre-heater, the one-level pre-heater pass through the pipeline with the bottom intercommunication of second grade pre-heater, low temperature steam condensate water in the low pressure steam condensate water buffer tank is in export outside to steam water tank after the heat transfer in the second grade pre-heater, the top of second grade pre-heater pass through the pipeline with the lower part intercommunication of tertiary pre-heater, concentrated hydrochloric acid in the second grade pre-heater pass through export to the upper portion of analytic tower after the tertiary heat exchanger heat transfer, the top of tertiary pre-heater pass through the pipeline with the top intercommunication of analytic tower, the upper portion of tertiary pre-heater pass through, The bottom of the analysis tower condenser is communicated with the bottom of the demister, and the lower part of the tertiary preheater is communicated with the lower part of the analysis tower condenser through a pipeline.
Further, the analysis tower condenser comprises an analysis tower first-stage condenser, an analysis tower second-stage condenser and an analysis tower third-stage condenser, and the demister comprises a first-stage demister and a second-stage demister; the top of the first-stage condenser of the desorption tower is communicated with the lower part of the third-stage preheater through a pipeline; the top of the second-stage condenser of the desorption tower is communicated with the lower part of the first-stage condenser of the desorption tower through a pipeline; the lower part of the first-stage demister is communicated with the lower part of the second-stage condenser of the desorption tower through a pipeline; the top of the third-stage condenser of the desorption tower is communicated with the top of the first-stage demister through a pipeline; the lower part of the second-stage demister is communicated with the lower part of the third-stage condenser of the desorption tower through a pipeline, and the dried hydrogen chloride gas is output through a pipeline at the top of the second-stage demister; the bottom of the first-stage condenser of the desorption tower, the second-stage condenser of the desorption tower, the third-stage condenser of the desorption tower, the first-stage demister and the second-stage demister is communicated with the upper parts of the desorption tower and the third-stage preheater through pipelines.
Further, the reboiler of the desorption tower comprises a reboiler of the desorption tower, a medium-pressure steam condensate buffer tank and a low-pressure steam flash tank, the top of the reboiler of the desorption tower is communicated with the lower part of the desorption tower through a pipeline, the medium-pressure steam is output to the upper part of the reboiler of the desorption tower, the top of the medium-pressure steam condensate buffer tank and the low-pressure steam flash tank through pipelines, the lower part of the medium-pressure steam condensate buffer tank is communicated with the lower part of the desorption tower reboiler through a pipeline, the bottom of the reboiler of the desorption tower is communicated with the bottom of the desorption tower through a pipeline, the bottom of the medium-pressure steam condensate buffer tank is communicated with the low-pressure steam flash tank through a pipeline, and the bottom of the low-pressure steam flash tank outputs low-pressure steam condensate water to the secondary preheater through a condensate water delivery pump, and the top of the low-pressure steam flash tank outputs the low-pressure steam condensate water to a dehydrating tower reboiler.
Further, the dehydration reboiling device comprises a dehydration tower reboiler and a low-pressure steam condensate buffer tank, the top of the dehydration tower reboiler is communicated with the lower part of the negative pressure dehydration tower through a pipeline, the lower part of the dehydration tower reboiler is communicated with the bottom of the negative pressure dehydration tower through a pipeline, the top of the low-pressure steam condensate buffer tank is communicated with the low-pressure steam flash tank and the upper part of the dehydration tower reboiler through a pipeline, low-pressure steam condensate water is output to the secondary preheater through the bottom of the low-pressure steam condensate buffer tank, and the lower part of the low-pressure steam condensate buffer tank is communicated with the lower part of the dehydration tower reboiler through a pipeline.
Furthermore, the upper portion of secondary preheater lets in low pressure steam condensate buffer tank and the low pressure steam condensate water in the low pressure steam flash tank, the lower part of secondary preheater is exported to the steam basin, waits to resolve concentrated hydrochloric acid and exports to the bottom of secondary preheater through the one-level preheater.
Further, the dilute acid water tank is connected with a sewage treatment station and the upper part of the negative pressure dehydration tower through pipelines, and the upper part of the negative pressure dehydration tower is connected with the dehydration tower condenser through a pipeline; and the dilute acid in the dilute acid buffer tank of the dehydration tower is sequentially output to the first-stage preheater and the dilute acid cooler of the desorption tower through a dilute hydrochloric acid delivery pump to the hydrogen chloride absorption process.
Compared with the prior art, the technical scheme of the utility model have following advantage:
(1) the utility model discloses a hydrochloric acid desorption device with negative pressure dehydration function, with the analytic technology combination of negative pressure dehydration technology and hydrochloric acid, with unnecessary water removal at the analytic in-process of hydrochloric acid, compare with traditional components of a whole that can function independently process design, reduction equipment investment and running cost that can be great can improve the utilization ratio of the energy through reasonable design simultaneously, the utility model discloses an analytic technology of hydrochloric acid does not receive impurity influence in the pending raw materials hydrochloric acid, can retrieve or get rid of the organic matter in the certain boiling point scope, compares 15 ~ 50% comprehensive energy consumption of saving with current components of a whole that can function independently design.
(2) The utility model discloses a hydrochloric acid resolving device with negative pressure dehydration function sets up waste heat recovery device, treats analytic concentrated hydrochloric acid and passes through in proper order the one-level pre-heater, the second grade pre-heater and tertiary pre-heater waste heat recovery step by step, treat analytic concentrated hydrochloric acid promptly with waste heat, the analytic tower of the hydrochloric acid of dehydration tower diluted acid buffer tank do not get into waste heat recovery step by step is carried out to waste heat of the dilute hydrochloric acid of negative pressure dehydration tower, the waste heat of low pressure steam condensate water in the low pressure steam flash tank, the waste heat of the steam condensate water in the low pressure steam condensate water buffer tank and the waste heat of the top of the tower mist of analytic tower get into after the analytic tower, make full use of waste heat reaches energy-conserving effect, and waste heat recovery treats analytic concentrated hydrochloric acid terminal point temperature control at 80 ~ 120 ℃, and preferred temperature interval control.
(3) The utility model discloses an analytic device of hydrochloric acid with negative pressure dehydration function, the steam condensate water warp of analytic tower reboiler the secondary steam that the low pressure steam flash tank produced gets into the dehydration reboiler carries out waste heat reutilization, reaches energy-conserving effect, the analytic tower negative pressure dehydration tower all adopts special high-efficient anticorrosive filler, reaches higher separation efficiency, reaches energy-conserving effect.
Drawings
The technical solution and the advantages of the present invention will be made apparent from the following detailed description of the embodiments of the present invention with reference to the accompanying drawings.
Fig. 1 is a structural diagram of a hydrochloric acid analyzer with negative pressure dehydration function according to an embodiment of the present invention;
fig. 2 is a flow chart illustrating a resolving process of a hydrochloric acid resolving device with a negative pressure dehydration function according to an embodiment of the present invention.
Reference numbers in the figures:
11 analytic tower, 12 tertiary preheaters, 13 analytic tower first grade condenser, 14 analytic tower second grade condenser, 15 analytic tower third grade condenser, 16 first grade defroster, 17 second grade defroster, 18 analytic tower dilute acid buffer tank, 21 negative pressure dehydration tower, 22 dehydration tower dilute acid buffer tank, 23 dehydration tower condenser, 24 vacuum unit, 25 dilute acid water tank, 26 dilute acid water delivery pump, 27 dilute hydrochloric acid delivery pump, 28 analytic tower dilute acid cooler, 31 analytic tower reboiler, 32 medium pressure steam condensate buffer tank, 33 low pressure steam flash tank, 34 condensate water delivery pump, 41 dehydration tower reboiler, 42 low pressure steam condensate buffer tank, 5 secondary preheaters, 6 primary preheaters.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those skilled in the art without creative efforts belong to the protection scope of the present invention.
The present embodiment provides a hydrochloric acid analyzer having a negative pressure dehydration function, as shown in fig. 1, including: the device comprises an analysis device, a negative pressure dehydration device and a waste heat recovery device, wherein the negative pressure dehydration device is communicated with the analysis device through a pipeline, and the waste heat recovery device is communicated with the analysis device and the negative pressure dehydration device through a pipeline.
The analysis device comprises an analysis tower 11, an analysis tower condenser, a demister, an analysis tower reboiling device and an analysis tower dilute acid buffer tank 18, wherein concentrated hydrochloric acid is conveyed to the top of the analysis tower 11 through a pump, mass transfer and heat transfer are carried out on mixed steam generated by heating the analysis tower reboiling device in the analysis tower 11, mixed gas obtained by escaping from the top of the analysis tower to the analysis tower condenser is obtained, and the mixed gas comprises hydrogen chloride gas, low-boiling-point organic matters and a small amount of water vapor. The operating pressure adaptive range of the analysis tower 11 is wide, the requirements for pressure resistance, temperature resistance, corrosion resistance and leakage resistance are high, and in order to overcome the use defects of pressure resistance, large thermal expansion coefficient, high leakage failure rate and the like of conventional anticorrosion equipment, a main cylinder body of the analysis tower 11 is made of high-strength fiber composite reinforced graphite, the main cylinder body is connected with a steel flange, the main cylinder body is connected with the steel flange through high-strength fiber composite, and the high-strength fiber is at least one of glass fiber, basalt fiber, aramid fiber, carbon fiber, silicon carbide fiber and silicon nitride fiber. The desorption tower 11 adopts high-efficiency corrosion-resistant filler, and the high-efficiency corrosion-resistant filler is at least one of porous graphite Raschig rings, porous graphite spherical filler, porous ceramic filler, tetrafluoro fiber filler and tetrafluoro regular filler. The types of binder substrates used in the material compounding process include, but are not limited to: one or more of furan resin, phenolic resin, silicon resin, epoxy resin, silicon carbon resin and silicon nitrogen resin. The top of the analysis tower condenser is communicated with the top of the analysis tower 11 through a pipeline, the lower part of the demister is communicated with the analysis tower condenser through a pipeline, dried hydrogen chloride gas is output through the top pipeline of the demister, and the mixed gas passes through the analysis tower condenser and the demister to remove moisture and low-boiling-point organic matters, so that the hydrogen chloride gas with high purity is obtained.
The bottom of the analysis tower condenser and the lower part of the demister are communicated with the analysis tower 11 through pipelines, and concentrated hydrochloric acid which is used for removing part of high-concentration organic matters behind the analysis tower condenser and the demister returns to the analysis tower 11 to continue analysis. The top of the reboiler of the desorption tower is communicated with the lower part of the desorption tower 11 through a pipeline, so that the mixed steam generated by heating is conveniently conveyed to the desorption tower 11 to transfer heat and mass with concentrated hydrochloric acid. The upper part of the dilute acid buffer tank 18 of the desorption tower is communicated with the lower part of the desorption tower 11 and the bottom of the desorption tower 11 through pipelines, so that the dilute acid in the desorption tower 11 is conveniently conveyed to the dilute acid buffer tank 18 of the desorption tower so as to enter a negative pressure dehydration process.
The negative pressure dehydration device is communicated with the bottom of the dilute acid buffer tank 18 of the desorption tower through a pipeline, the negative pressure dehydration device comprises a negative pressure dehydration tower 21, a dehydration tower dilute acid buffer tank 22, a dehydration tower condenser 23, a vacuum unit 24, a dilute acid water tank 25 and a dehydration reboiling device, the upper part of the negative pressure dehydration tower 21 is communicated with the bottom of the dilute acid buffer tank 18 of the desorption tower through a pipeline, the lower part of the dehydration tower dilute acid buffer tank 22 is communicated with the bottom of the negative pressure dehydration tower 21, the top of the dehydration tower condenser 23 is communicated with the top of the negative pressure dehydration tower 21 through a pipeline, the constant boiling dilute hydrochloric acid coming out of the kettle of the desorption tower 11 enters the negative pressure dehydration tower 21 according to the size of the dehydration water quantity, the constant boiling dilute hydrochloric acid enters the negative pressure dehydration tower 21 to be subjected to hydrochloric acid flash evaporation cooling, and steam generated by heating of the kettle of the negative pressure dehydration tower 21 and reflux acid water at the top are subjected to heat transfer in the tower of, And (4) transferring mass and separating out acid water containing trace hydrogen chloride. The dilute hydrochloric acid which does not enter the negative pressure dehydration tower and the raw material hydrochloric acid which enters the desorption tower exchange heat in a two-phase mode and then enter other working procedures of a factory to continuously absorb the hydrogen chloride. The vacuum unit 24 is communicated with the lower part of the dehydrating tower condenser 23 through a pipeline, and the dilute acid water tank 25 is communicated with the bottom of the dehydrating tower condenser 23 through a pipeline. A part of dilute acid in the dilute acid water tank 25 is output to a sewage treatment station through a dilute acid water delivery pump 26, the other part of dilute acid in the dilute acid water tank 25 is delivered to the upper part of the negative pressure dehydration tower 21 as a reflux liquid of the dehydration tower, and the upper part of the negative pressure dehydration tower 21 is connected with the dehydration tower condenser 23 through a pipeline. And water drops of the water vapor at the upper part of the negative pressure dehydration tower 21 under the action of gravity are output to the sewage treatment station through a pipeline. The dehydration reboiling device is communicated with the lower part and the bottom of the negative pressure dehydration tower 21 through pipelines. The negative pressure dehydration tower 21 needs to be resistant to negative pressure, corrosion and leakage and overcomes the defects of conventional materials, the negative pressure dehydration tower 21 adopts a steel composite enamel component coating, the component material of the steel composite enamel component coating is at least one of silicon dioxide, aluminum oxide, zirconium oxide, a binder, polyamide resin, polyimide resin, polytetrafluoroethylene resin, silicon nitrogen resin and polyether resin, and the steel composite enamel component coating is prepared by adopting a thermal spraying process. The negative pressure dehydration tower 21 adopts high-efficiency corrosion-resistant filler, the high-efficiency corrosion-resistant filler is at least one of porous graphite Raschig rings, porous graphite spherical filler, porous ceramic filler, tetrafluoro fiber filler and tetrafluoro regular filler, and the types of the used binder base materials include but are not limited to: one or more of furan resin, phenolic resin, silicon resin, epoxy resin, silicon carbon resin and silicon nitrogen resin. The negative pressure dehydration tower 21 adopts high-efficiency corrosion-resistant filler, so that the number of theoretical plates of the filler per meter can be increased, the separation efficiency is also increased, the reflux ratio can be reduced by 10-30%, and the energy-saving effect is achieved.
The waste heat recovery device comprises a primary preheater 6, a secondary preheater 5 and a tertiary preheater 12, the dilute acid in the dilute acid buffer tank 22 of the dehydration tower exchanges heat in the first-stage preheater 6 and then is output to the hydrogen chloride absorption process through the dilute acid cooler 28 of the desorption tower, the primary preheater 6 is communicated with the bottom of the secondary preheater 5 through a pipeline, the low-temperature steam condensate in the low-pressure steam condensate buffer tank 42 is subjected to heat exchange in the secondary preheater 5 and then is output to an outdoor steam water tank, the top of the secondary preheater 5 is communicated with the lower part of the tertiary preheater 12 through a pipe, concentrated hydrochloric acid in the secondary preheater 5 is output to the upper part of the desorption tower 11 after heat exchange by the tertiary heat exchanger 12, the top of the tertiary preheater 12 is communicated with the top of the desorption tower 11 through a pipeline, the lower part of the tertiary preheater 12 is communicated with the lower part of the desorption tower condenser through a pipeline. The upper part of the tertiary preheater 12 is communicated with the upper part of the desorption tower 11, the bottom of the desorption tower condenser and the bottom of the demister through pipelines.
The analysis tower condenser comprises an analysis tower first-stage condenser 13, an analysis tower second-stage condenser 14 and an analysis tower third-stage condenser 15, and the demister comprises a first-stage demister 16 and a second-stage demister 17. The top of the analysis tower first-stage condenser 13 is communicated with the lower part of the third-stage preheater 12 through a pipeline, the top of the analysis tower second-stage condenser 14 is communicated with the lower part of the analysis tower first-stage condenser 13 through a pipeline, the lower part of the first-stage demister 16 is communicated with the lower part of the analysis tower second-stage condenser 14 through a pipeline, the top of the analysis tower third-stage condenser 15 is communicated with the top of the first-stage demister 16 through a pipeline, the lower part of the second-stage demister 17 is communicated with the lower part of the analysis tower third-stage condenser 15 through a pipeline, and dried hydrogen chloride gas passes through the pipeline at the top of the second-stage demister 17 to. The bottoms of the desorption tower first-stage condenser 13, the desorption tower second-stage condenser 14, the desorption tower third-stage condenser 15, the first-stage demister 16, and the second-stage demister 17 are communicated with the upper portions of the desorption tower 11 and the third-stage preheater 12 through pipes. If the hydrochloric acid to be treated contains low-boiling-point organic matters, controlling different condensation temperatures of the mixed gas escaped from the top of the desorption tower 11, intermittently discharging concentrated hydrochloric acid solution containing the low-boiling-point organic matters through a sectional condensation method, returning the concentrated hydrochloric acid solution to a user process, and finally, freezing, separating and drying the hydrogen chloride gas to obtain the product. And controlling the system pressure of the desorption tower 11 to be an optimal value, obtaining constant boiling acid with a certain concentration at the tower kettle, and forming a linear relation between the acid outlet concentration of the constant boiling acid and the working pressure of the desorption tower. The concentrated hydrochloric acid to be analyzed contains lower alcohol or other low-boiling point organic matters, calcium ions, sulfate ions, silicon dioxide, other heavy metal ions, high-boiling point organic matters, organic sulfonate and other impurities. The optimal sectional condensation temperature of the lower alcohol or the low-boiling-point organic matter is determined according to the type and the content of the lower alcohol or the low-boiling-point organic matter, and the optimal condensation temperature range is calculated according to the boiling point of the mixed gas component at the top of the desorption tower under normal pressure as follows: the preferable discharge positions of concentrated hydrochloric acid containing low-boiling point organic matters are that: after the secondary condenser 14.
The reboiler of the desorption tower comprises a reboiler 31 of the desorption tower, a medium pressure steam condensate buffer tank 32 and a low pressure steam flash tank 33, wherein the top of the reboiler 31 of the desorption tower is communicated with the lower part of the desorption tower 11 through a pipeline, medium pressure steam is output to the upper part of the reboiler 31 of the desorption tower, the top of the medium pressure steam condensate buffer tank 32 and the low pressure steam flash tank 33 through a pipeline, the lower part of the medium pressure steam condensate buffer tank 32 is communicated with the lower part of the reboiler 31 of the desorption tower through a pipeline, the bottom of the reboiler 31 of the desorption tower is communicated with the bottom of the desorption tower 11 through a pipeline, the bottom of the medium pressure steam condensate buffer tank 32 is communicated with the low pressure steam flash tank 33 through a pipeline, and the bottom of the low pressure steam flash tank 33 outputs low pressure steam condensate to the secondary preheater 5 through a condensate transfer pump 34, the overhead vapor of the low pressure steam flash drum 33 is output to a dehydration column reboiler 41.
The dehydration reboiling device comprises a dehydration tower reboiler 41 and a low-pressure steam condensate buffer tank 42, the top of the dehydration tower reboiler 41 is communicated with the lower part of the negative pressure dehydration tower 21 through a pipeline, the lower part of the dehydration tower reboiler is communicated with the bottom of the negative pressure dehydration tower through a pipeline, the top of the low-pressure steam condensate buffer tank 42 is communicated with the low-pressure steam flash tank 33 and the upper part of the dehydration tower reboiler 41 through a pipeline, low-pressure steam condensate water is output to the secondary preheater 5 from the bottom of the low-pressure steam condensate buffer tank 42, and the lower part of the low-pressure steam condensate buffer tank 42 is communicated with the lower part of the dehydration tower reboiler 41 through a pipeline. The upper portion of secondary preheater 5 lets in low pressure steam condensate buffer tank 42 and the low pressure steam condensate water in the low pressure steam flash tank 33, the lower part of secondary preheater 5 is exported to the steam basin, waits to resolve concentrated hydrochloric acid and exports to the bottom of secondary preheater 5 through one-level preheater 6. The dilute acid in the dilute acid buffer tank 22 of the dehydration tower is sequentially output to the first-stage preheater 6 and the dilute acid cooler 28 of the desorption tower through a dilute hydrochloric acid delivery pump 27 to the hydrogen chloride absorption process.
As shown in fig. 2, the hydrochloric acid desorption process of the hydrochloric acid desorption device with negative pressure dehydration function of the present invention includes the following steps: s10 concentrated hydrochloric acid is pumped to the top of the desorber 11 where it undergoes mass and heat transfer with the mixed vapor produced by the desorber reboiling equipment to produce a mixed gas and dilute acid. And S20, allowing the mixed gas to escape from the top of the desorption tower 11 to the tertiary preheater 12, and allowing the mixed gas to pass through a desorption tower condenser and the demister in sequence to remove redundant moisture and low-boiling-point organic matters to obtain hydrogen chloride gas for later use. S30 the dilute acid is transported to the dilute acid buffer tank 18 from the lower part of the desorption tower 11, and is pumped to the negative pressure dehydration device by the dilute acid buffer tank 18 to separate the dilute acid water containing trace hydrogen chloride to a sewage treatment station. The pressure operation range of the desorption tower 11 is 0-1.0 Mpa, and the operation pressure range of the negative pressure dehydration tower 21 is-0.1-0 Mpa.
The utility model discloses do not regard as the target with the whole separation of hydrogen chloride and water in waiting to resolve the concentrated hydrochloric acid, but based on the basis that hydrochloric acid often resolves, the appropriate amount water of desorption, the desorption water yield scope is 0 ~ 30% of the dilute hydrochloric acid flow of resolution tower cauldron.
The S10 concentrated hydrochloric acid is pumped to the top of the desorber 11 where it undergoes mass and heat transfer with the mixed vapor produced by the desorber reboiling equipment to produce a mixed gas and dilute acid.
The process for preparing the dry hydrogen chloride gas by using the S20 mixed gas comprises the following steps:
the mixed gas sequentially passes through the top of the analysis tower 11, the third-stage preheater 12, the first-stage condenser 13 of the analysis tower, the second-stage condenser 14 of the analysis tower, the first-stage demister 16, the third-stage condenser 15 of the analysis tower and the second-stage demister 17 to obtain dry hydrogen chloride gas. Part of the liquid water carried by the mixed gas when entering the tertiary preheater 12 is returned to the desorption tower 11 through a pipeline. The third-stage preheater 12, the first-stage condenser 13 of the desorption tower, the second-stage condenser 14 of the desorption tower, the first-stage demister 16, the third-stage condenser 15 of the desorption tower and the concentrated hydrochloric acid solution containing a small amount of organic matters, which is separated in the drying process of the second-stage demister 17, are returned to the desorption tower 11 through a pipeline. The condensate of the second-stage condenser 14 or the third-stage condenser 15 of the desorption tower is subjected to condensation temperature control according to the boiling point of organic matters contained in the mixed gas, and the condensate is discharged from the clearance.
In the S30, the pressure operation range of the desorption tower 11 is preferably 0.2 to 0.6MPa, and the operation pressure range of the negative pressure dehydration tower 21 is preferably-0.09 to-0.07 MPa.
The dehydration process of the negative pressure dehydration device in the step S30 is as follows:
the dilute acid in the desorption tower 11 is output to the dilute acid buffer tank 18 of the desorption tower, the dilute acid in the dilute acid buffer tank 18 of the desorption tower is pumped to the upper part of the negative pressure dehydration tower 21, the dilute acid in the negative pressure dehydration tower 21 and the mixed steam generated by the reboiling device of the dehydration tower perform mass transfer and heat transfer to generate a second mixed gas carrying water vapor, the second mixed gas enters the dilute acid water tank 25 after being cooled by the dehydration tower condenser 23, because the concentration of the hydrochloric acid in the dilute acid water tank 25 is very low, a part of the dilute acid in the dilute acid water tank 25 is output to a sewage treatment station through the dilute acid water delivery pump 26, and the other part of the dilute acid in the dilute acid water tank 25 is delivered to the upper part of the negative pressure dehydration tower 21 as the dehydration tower dehydration liquid. The dilute acid output from the bottom of the negative pressure dehydration tower 21 enters the dehydration tower dilute acid buffer tank 22, is pumped to the primary preheater 6 for waste heat recovery, is cooled by the desorption tower dilute acid cooler 28 after heat transfer, and is output to the hydrogen chloride absorption process.
The process for recovering the waste heat by using the waste heat recovery device comprises the following steps:
and recovering the residual heat of the hydrochloric acid in the dilute acid buffer tank 22 of the dehydrating tower and the residual heat of the dilute hydrochloric acid which does not enter the negative pressure dehydrating tower 21 by the desorption tower through the primary preheater 6, recovering the residual heat of the low-pressure steam condensate water in the low-pressure steam flash tank 33 and the residual heat of the steam condensate water in the low-pressure steam condensate water buffer tank 42 in the secondary preheater 5, then entering the tertiary preheater 12, and recovering the residual heat of the tower top mixed gas of the desorption tower 11 in the tertiary preheater 12 to form a steam-liquid mixture or a high-temperature liquid-phase material. The material after waste heat recovery returns to the desorption tower 11 through a pipeline, vapor-liquid separation is carried out in the desorption tower, the formed mixed gas and the mixed gas in the desorption tower 11 enter a three-stage preheater 12, and liquid flows downwards in the desorption tower 11 to continuously carry out mass transfer and heat transfer.
Example 1
The concentrated hydrochloric acid with 31 percent of ethanol to be treated contains 0.1 percent of ethanol, the treatment capacity is 20t/h, the hydrogen chloride gas is required to be analyzed by adopting the conventional analysis, the redundant water is removed at the same time for 1t/h, a water station is decontaminated, and about 20 percent of diluted hydrochloric acid after the analysis is returned to other working procedures of a factory.
In the embodiment, the hydrochloric acid to be treated contains ethanol, and the ethanol reacts with the entrainer for conventional deep analysis such as calcium chloride and magnesium chloride, so that the hydrochloric acid is not suitable for removing excessive water by the conventional calcium chloride method, the hydrochloric acid is treated by the calcium chloride method, and the comprehensive steam consumption is about 5.7 t/h; the excess water is removed by deep analysis by adopting a differential pressure method, the investment is large, the operation cost is high, and the comprehensive steam consumption is about 7.5 t/h.
Adopt the utility model discloses hydrochloric acid resolving device with negative pressure dehydration function resolves, pending hydrochloric acid gets into resolving tower 11, owing to do not introduce broken azeotropic agent, insensitive to ethanol impurity, hydrogen chloride, water, ethanol mist follow the top of the tower of resolving tower 11 escapes, resolving tower 11 operating pressure control is at 0.3MPa (G), dilute hydrochloric acid 16t/h about 18.5% of the tower cauldron of resolving tower 11 gets into negative pressure dehydration tower 21, remaining tower cauldron dilute acid with negative pressure dehydration tower 21 gets into the one-level preheater 6 together, the operating pressure of negative pressure dehydration tower 21 is-0.085 MPa (G), resolving tower 11, negative pressure dehydration tower 21 packs and adopts porous graphite spherical packing and the regular packing combination of tetrafluoro, negative pressure dehydration tower 21 reflux ratio 0.9, the top of the tower evaporates out water 1t/h, the tower cauldron of negative pressure dehydration tower 21 goes out acid concentration 19.7%, the comprehensive steam consumption is 4.7 t/h. The comprehensive energy-saving efficiency reaches more than 20 percent.
The hydrochloric acid from the primary preheater 6 enters the secondary preheater 5 for double-effect heat exchange with the low-pressure steam condensate water, the hydrochloric acid after heat exchange continues to enter the tertiary preheater 12 for double-effect heat exchange with the gas phase at the top of the desorption tower 11 and then enters the desorption tower 11, and the preheated end point temperature is controlled to be about 98 ℃.
Controlling the temperature of the gas phase at the top of the desorption tower at 45 ℃ in the first-stage condenser 13, controlling the temperature of the second-stage condenser 14 of the desorption tower at-6 ℃, and extracting concentrated hydrochloric acid containing ethanol from a liquid phase outlet of a gas-liquid separator 14 of the second-stage condenser of the desorption tower.
The graphite cylinder of the desorption tower 11 is reinforced by carbon fiber composite, the connection part of the cylinder connecting flange is formed by locally compounding aramid fiber, and then the carbon fiber is integrally compounded, and the carbon fiber, the aramid fiber, the steel flange and the graphite are bonded into a whole by using the modified phenolic resin as a base material.
The negative pressure dehydration tower 21 adopts an enamel-like component composite coating, and comprises the following components: silica, a binder, zirconia, and polytetrafluoroethylene resin.
Example 2
The concentration of concentrated hydrochloric acid to be treated is 28%, a small amount of silicon dioxide is contained, the treatment capacity is 36.4t/h, hydrochloric acid is normally analyzed, hydrogen chloride gas reaches the use point, meanwhile, 3t/h of material balance excess water is evaporated, and dilute hydrochloric acid returns to other procedures to absorb hydrogen chloride, so that a closed cycle is formed.
The concentrated hydrochloric acid to be treated in the embodiment contains silicon dioxide, and calcium chloride or magnesium chloride and other azeotrope breaking agents are adopted for deep analysis, so that the silicon dioxide can generate silicate precipitates and accumulate in the environment of the concentrated hydrochloric acid, and serious influence is caused on long-period production.
When equal amount of hydrogen chloride is analyzed and equal amount of water is removed, the calcium chloride method is adopted for treatment, the comprehensive steam consumption is about 11t/h, and the differential pressure method is adopted for treatment, the comprehensive steam consumption is about 15 t/h.
The hydrochloric acid analysis device with the negative pressure dehydration function of the utility model is adopted for analysis, concentrated hydrochloric acid to be processed enters the analysis tower 11, because no entrainer is introduced, a small amount of silicon dioxide can not be deposited in the system, the mixed gas of hydrogen chloride and water escapes from the top of the tower and is dried by multi-stage condensation, the operation pressure of the analysis tower 11 is controlled at 0.7MPa (G), about 31.2t/h of dilute hydrochloric acid at the tower bottom of the analysis tower 11 is about 16.1 percent to enter the negative pressure dehydration tower 21, the rest dilute acid at the tower bottom of the negative pressure dehydration tower 21 enters the primary preheater 6, the operation pressure of the negative pressure dehydration tower 21 is-0.085 MPa (G), the analysis tower 11 and the negative pressure dehydration tower 21 are filled with porous tetrafluoro fiber, porous graphite Raschig rings and tetrafluoro structured packing, the reflux ratio of the negative pressure dehydration tower 21 is 0.7, the top of the tower is evaporated with 3t/h of water, the concentration of the acid discharged from the tower bottom is about 17.8 percent, the acid is converted into the equivalent hydrogen chloride and the equivalent water removal, and the comprehensive steam consumption is about 8.0 t/h. The comprehensive energy-saving efficiency reaches more than 37.5 percent. The pressure of the analytical tower is improved and the energy-saving effect is linear and obvious.
The hydrochloric acid from the primary preheater 6 enters the secondary preheater 5 for double-effect heat exchange with the low-pressure steam condensate water, the hydrochloric acid after heat exchange continues to enter the tertiary preheater 12 for double-effect heat exchange with the top gas phase of the desorption tower 11 and then enters the desorption tower 11, and the preheated end point temperature is controlled to be about 90 ℃.
The graphite cylinder of the desorption tower 11 is reinforced by compounding glass fibers, the basalt fibers are firstly compounded locally at the connection part of the cylinder connection flange, then the glass fibers are compounded integrally, and the glass fibers, the basalt fibers, the steel flange and the graphite are bonded into a whole by using epoxy resin as a base material as a binder.
The negative pressure dehydration tower 21 adopts an enamel-like component composite coating, and comprises the following components: silicon dioxide, a binder, aluminum oxide and polyether resin.
The above is only the exemplary embodiment of the present invention, and not the limitation of the present invention, all the equivalent structures or equivalent processes of the present invention are used, or directly or indirectly applied to other related technical fields, and the same principle is included in the patent protection scope of the present invention.
Claims (7)
1. A hydrochloric acid analysis device with negative pressure dehydration function is characterized by comprising an analysis device and a negative pressure dehydration device,
the analysis device comprises an analysis tower (11), an analysis tower condenser, a demister, an analysis tower reboiling device and an analysis tower diluted acid buffer tank (18), wherein the top of the analysis tower condenser is communicated with the top of the analysis tower (11) through a pipeline, the lower part of the demister is communicated with the analysis tower condenser through a pipeline, dried hydrogen chloride gas is output through the pipeline at the top of the demister, the bottom of the analysis tower condenser and the lower part of the demister are communicated with the upper part of the analysis tower (11) through pipelines, the top of the analysis tower reboiling device is communicated with the lower part of the analysis tower (11) through a pipeline, and the upper part of the analysis tower diluted acid buffer tank (18) is communicated with the lower part of the analysis tower (11) and the bottom of the analysis tower (11) through a pipeline;
the negative pressure dehydration device is communicated with the bottom of the analysis tower dilute acid buffer tank (18) through a pipeline, the negative pressure dehydration device comprises a negative pressure dehydration tower (21), a dehydration tower dilute acid buffer tank (22), a dehydration tower condenser (23), a vacuum unit (24), a dilute acid water tank (25) and a dehydration reboiling device, the upper part of the negative pressure dehydration tower (21) is communicated with the bottom of the analysis tower dilute acid buffer tank (18) through a pipeline, the lower part of the dehydration tower dilute acid buffer tank (22) is communicated with the bottom of the negative pressure dehydration tower (21), the top of the dehydration tower condenser (23) is communicated with the top of the negative pressure dehydration tower (21) through a pipeline, the vacuum unit (24) is communicated with the lower part of the dehydration tower condenser (23) through a pipeline, and the dilute acid water tank (25) is communicated with the bottom of the dehydration tower condenser (23) through a pipeline, the dehydration reboiling device is communicated with the lower part and the bottom of the negative pressure dehydration tower (21) through pipelines.
2. The hydrochloric acid desorption device with the negative pressure dehydration function as claimed in claim 1, further comprising a waste heat recovery device, comprising a primary preheater (6), a secondary preheater (5) and a tertiary preheater (12), wherein the dilute acid in the dilute acid buffer tank (22) of the dehydration tower is subjected to heat exchange in the primary preheater (6) and then is output to a hydrogen chloride absorption process through a dilute acid cooler (28) of the desorption tower, the primary preheater (6) is communicated with the bottom of the secondary preheater (5) through a pipeline, the low-temperature steam condensate water in the low-pressure steam condensate buffer tank (42) is subjected to heat exchange in the secondary preheater (5) and then is output to an outdoor steam water tank, the top of the secondary preheater (5) is communicated with the lower part of the tertiary preheater (12) through a pipeline, and the concentrated hydrochloric acid in the secondary preheater (5) is subjected to heat exchange through the tertiary heat exchanger and then is output to the upper part of the desorption tower (11), the top of the three-stage preheater (12) is communicated with the top of the analysis tower (11) through a pipeline, the upper part of the three-stage preheater (12) is communicated with the upper part of the analysis tower (11), the bottom of the analysis tower condenser and the bottom of the demister through pipelines, and the lower part of the three-stage preheater (12) is communicated with the lower part of the analysis tower condenser through a pipeline.
3. The hydrochloric acid desorption device with negative pressure dehydration function as claimed in claim 2, characterized in that the desorption tower condenser comprises a desorption tower primary condenser (13), a desorption tower secondary condenser (14) and a desorption tower tertiary condenser (15), and the demister comprises a primary demister (16) and a secondary demister (17);
the top of the first-stage condenser (13) of the desorption tower is communicated with the lower part of the third-stage preheater (12) through a pipeline;
the top of the second-stage condenser (14) of the desorption tower is communicated with the lower part of the first-stage condenser (13) of the desorption tower through a pipeline;
the lower part of the first-stage demister (16) is communicated with the lower part of the second-stage condenser (14) of the desorption tower through a pipeline;
the top of the tertiary condenser (15) of the desorption tower is communicated with the top of the primary demister (16) through a pipeline;
the lower part of the secondary demister (17) is communicated with the lower part of the tertiary condenser (15) of the desorption tower through a pipeline, and the dried hydrogen chloride gas is output through the pipeline at the top of the secondary demister (17);
the bottom of the first-stage condenser (13) of the desorption tower, the second-stage condenser (14) of the desorption tower, the third-stage condenser (15) of the desorption tower, the first-stage demister (16) and the second-stage demister (17) are communicated with the upper parts of the desorption tower (11) and the third-stage preheater (12) through pipelines.
4. The hydrochloric acid desorption apparatus with negative pressure dehydration function as claimed in claim 2, wherein the desorption tower reboiling apparatus comprises a desorption tower reboiler (31), an intermediate pressure steam condensate buffer tank (32) and a low pressure steam flash drum (33), the top of the desorption tower reboiler (31) is communicated with the lower part of the desorption tower (11) through a pipeline, the intermediate pressure steam is output to the upper part of the desorption tower reboiler (31), the top of the intermediate pressure steam condensate buffer tank (32) and the low pressure steam flash drum (33) through a pipeline, the lower part of the intermediate pressure steam condensate buffer tank (32) is communicated with the lower part of the desorption tower reboiler (31) through a pipeline, the bottom of the desorption tower reboiler (31) is communicated with the bottom of the desorption tower (11) through a pipeline, and the bottom of the intermediate pressure steam condensate buffer tank (32) is communicated with the low pressure steam flash drum (33) through a pipeline, the bottom of the low pressure steam flash tank (33) outputs low pressure steam condensate to the secondary preheater (5) via a condensate transfer pump (34), and the top of the low pressure steam flash tank (33) outputs to a dehydration column reboiler (41).
5. The hydrochloric acid desorption device with negative pressure dehydration function as claimed in claim 4, the dehydration reboiling device comprises the dehydration tower reboiler (41) and a low-pressure steam condensate buffer tank (42), the top of the dehydrating tower reboiler (41) is communicated with the lower part of the negative pressure dehydrating tower (21) through a pipeline, the lower part of the dehydrating tower reboiler (41) is communicated with the bottom of the negative pressure dehydrating tower (21) through a pipeline, the top of the low-pressure steam condensate buffer tank (42) is communicated with the low-pressure steam flash tank (33) and the upper part of the dehydrating tower reboiler (41) through pipelines, the bottom of the low-pressure steam condensate buffer tank (42) outputs low-pressure steam condensate to the secondary preheater (5), the lower part of the low-pressure steam condensate buffer tank (42) is communicated with the lower part of the dehydrating tower reboiler (41) through a pipeline.
6. The hydrochloric acid desorption device with the negative pressure dehydration function as claimed in claim 4, wherein the upper part of the secondary preheater (5) is introduced into the low pressure steam condensate buffer tank (42) and the low pressure steam condensate in the low pressure steam flash tank (33), the lower part of the secondary preheater (5) is output to a steam water tank, and concentrated hydrochloric acid to be desorbed is output to the bottom of the secondary preheater (5) through the primary preheater (6).
7. The hydrochloric acid desorption device with negative pressure dehydration function as claimed in claim 2,
the diluted acid water tank (25) is connected with a sewage treatment station and the upper part of the negative pressure dehydration tower (21) through pipelines, and the upper part of the negative pressure dehydration tower (21) is connected with the dehydration tower condenser (23) through a pipeline;
and dilute acid in the dilute acid buffer tank (22) of the dehydration tower is sequentially output to the first-stage preheater (6) and the dilute acid cooler (28) of the desorption tower through a dilute hydrochloric acid delivery pump (27) to a hydrogen chloride absorption process.
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